JP2003063823A - Indium - tin - oxide, method for manufacturing the same and the use - Google Patents

Indium - tin - oxide, method for manufacturing the same and the use

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Publication number
JP2003063823A
JP2003063823A JP2002177650A JP2002177650A JP2003063823A JP 2003063823 A JP2003063823 A JP 2003063823A JP 2002177650 A JP2002177650 A JP 2002177650A JP 2002177650 A JP2002177650 A JP 2002177650A JP 2003063823 A JP2003063823 A JP 2003063823A
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Prior art keywords
indium
tin
oxide
solution
salt
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
JP2002177650A
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Japanese (ja)
Inventor
Sabine Servaty
ザーファティ ザビーネ
Guenther Michael
ミヒャエル ギュンター
Christiane Heyer
ハイヤー クリスティアーネ
Stipan Katusic
カトゥジック シュティパン
Horst Miess
ミース ホルスト
Peter Kress
クレス ペーター
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Evonik Operations GmbH
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Degussa GmbH
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Publication date
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Publication of JP2003063823A publication Critical patent/JP2003063823A/en
Withdrawn legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
    • H01B1/08—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances oxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G19/00—Compounds of tin
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/14—Pore volume

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Organic Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Inorganic Chemistry (AREA)
  • Composite Materials (AREA)
  • Physics & Mathematics (AREA)
  • Paints Or Removers (AREA)
  • Catalysts (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Conductive Materials (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

PROBLEM TO BE SOLVED: To obtain indium - tin - oxide capable of coating on plastics. SOLUTION: This indium - tin - oxide is characterized by having 1 to 200 nm of the average primary particle size, 0.1 to 300 m<2> /g of BET surface area, a cubic crystal of indium oxide, a tetragonal crystal of tin oxide, 0.03 to 0.30 mL/g of mesopore measured by a BJH method, 1.5 to 5.0 mL/g of macropore 50 to 2,000 g/L of the bulk density. This indium - tin - oxide is manufactured by mixing an indium salt solution with a tin salt solution, spraying the mixture, and thermally decomposing the sprayed mixture and used for manufacturing transparent and conductive coatings and coating films.

Description

【発明の詳細な説明】Detailed Description of the Invention

【０００１】[0001]

【発明の属する技術分野】本発明はインジウム−錫−酸
化物、その製造方法および使用に関する。FIELD OF THE INVENTION The present invention relates to indium-tin-oxides, their method of preparation and use.

【０００２】[0002]

【従来の技術】インジウム−錫−酸化物は導電性の表面
被覆、例えばガラス板に使用される。Indium-tin-oxide is used for electrically conductive surface coatings such as glass plates.

【０００３】インジウムおよび錫の加水分解可能な化合
物の溶液にガラス板を浸漬し、乾燥し、引き続き５５０
℃までの温度で焼成することにより、ガラス板にインジ
ウム−錫酸化物を被覆することは知られている（米国特
許第４５６８５７８号）。公知の方法は、この方法を使
用して、例えばプラスチックを被覆できないという欠点
を有する。The glass plate is dipped in a solution of the hydrolyzable compound of indium and tin, dried and then 550
It is known to coat glass plates with indium-tin oxide by firing at temperatures up to ° C (US Pat. No. 4,568,578). The known method has the disadvantage that it cannot be used, for example, to coat plastics.

【０００４】[0004]

【発明が解決しようとする課題】従ってプラスチックを
インジウム−錫−酸化物で被覆するという課題が存在す
る。The problem therefore exists of coating plastics with indium-tin-oxide.

【０００５】[0005]

【課題を解決するための手段】前記課題は、本発明によ
り解決される。The above problems are solved by the present invention.

【０００６】本発明の対象は、以下の物理的化学的パラ
メーター：透過型電子顕微鏡（ＴＥＭ）により決定した 平均的一次粒子の大きさ １〜２００ｎｍ、 ＢＥＴ表面積（ＤＩＮ６６１３１） ０.１〜３００ｍ２／ｇ、 Ｘ線回折法（ＸＲＤ）による構造 立方晶の酸化インジウム 正方晶の酸化錫、 ＢＪＨ法（ＤＩＮ６６１３４）による メソポア ０.０３〜０.３０ｍｌ／ｇ、 マクロポア（ＤＩＮ６６１３３） １.５〜５.０ｍｌ／ｇ、 かさ密度（ＤＩＮ−ＩＳＯ７８７／ＸＩ） ５０〜２０００ｇ／ｌ を特徴とするインジウム−錫−酸化物である。The subject of the invention is the following physicochemical parameters: average primary particle size determined by transmission electron microscopy (TEM) 1-200 nm, BET surface area (DIN 66131) 0.1-300 m 2 / g, structure by X-ray diffraction method (XRD) cubic indium oxide tetragonal tin oxide, mesopores by BJH method (DIN66134) 0.03 to 0.30 ml / g, macropores (DIN66133) 1.5 to 5.0 ml / G, bulk density (DIN-ISO787 / XI) 50-2000 g / l indium-tin-oxide.

【０００７】本発明のインジウム−錫−酸化物は、酸化
物および／または元素の金属の形の以下の物質が組み込
まれていてもよく、The indium-tin-oxide of the present invention may incorporate the following substances in the form of oxides and / or elemental metals:

【０００８】[0008]

【表１】 [Table 1]

【０００９】この場合に出発物質として相当する塩を使
用することができる。Corresponding salts can be used as starting materials in this case.

【００１０】本発明のもう１つの対象は、本発明による
インジウム−錫−酸化物の製造方法であり、インジウム
塩の溶液を錫塩の溶液と混合し、場合により少なくとも
１種のドーピング成分の溶液を添加し、この溶液混合物
を噴霧し、噴霧した溶液混合物を熱分解し、得られた生
成物を排ガスから分離することを特徴とする。Another subject of the invention is a process for the preparation of indium-tin oxide according to the invention, in which a solution of indium salt is mixed with a solution of tin salt, optionally with a solution of at least one doping component. Is added, the solution mixture is sprayed, the sprayed solution mixture is pyrolyzed, and the product obtained is separated from the exhaust gas.

【００１１】塩として、無機化合物、例えば塩化物、硝
酸塩および金属有機前駆物質、例えば酢酸塩、アルコラ
ートを使用することができる。As salts, it is possible to use inorganic compounds such as chlorides, nitrates and metal organic precursors such as acetates, alcoholates.

【００１２】溶液混合物は、場合により疎水化されてい
てもよい、熱分解により製造される珪酸の分散液または
珪酸ゾル（シリカゾル）を付加的に含有することができ
る。この場合に珪酸が結晶核として機能し、従って珪酸
の最大粒度は最終生成物の最大粒度により決定される。The solution mixture may additionally contain a pyrolytically prepared dispersion of silicic acid or a silicic acid sol (silica sol), which may optionally be hydrophobized. In this case, silicic acid functions as crystal nuclei, so that the maximum particle size of silicic acid is determined by the maximum particle size of the final product.

【００１３】溶液は、場合により水、アルコール、例え
ばエタノール、プロパノールおよび／またはアセトンの
ような水溶性有機溶剤を含有することができる。The solution may optionally contain water, alcohols, water-soluble organic solvents such as ethanol, propanol and / or acetone.

【００１４】溶液の噴霧は超音波噴霧器、超音波吹き付
け器、二成分ノズルまたは三成分ノズルを用いて行うこ
とができる。超音波噴霧器または超音波吹き付け器を使
用する場合は、得られたエーロゾルを、火炎に供給する
キャリアガスおよび／またはＮ２／Ｏ２空気と混合する
ことができる。The solution can be sprayed using an ultrasonic sprayer, an ultrasonic sprayer, a two-component nozzle or a three-component nozzle. When using an ultrasonic nebulizer or an ultrasonic spray device is obtained aerosol can be mixed with a carrier gas and / or N 2 / O 2 air supplied to the flame.

【００１５】二成分ノズルまたは三成分ノズルを使用す
る場合は、エーロゾルを直接火炎に噴霧することができ
る。When using a two-component or three-component nozzle, the aerosol can be sprayed directly onto the flame.

【００１６】水と混合不可能の有機溶剤、例えばエーテ
ルも使用することができる。It is also possible to use organic solvents which are immiscible with water, for example ethers.

【００１７】分離はフィルターまたはサイクロンを用い
て行うことができる。Separation can be carried out using filters or cyclones.

【００１８】熱分解は、水素／空気および酸素の燃焼に
より生じる火炎中で行うことができる。水素の代わりに
メタン、ブタンおよびプロパンを使用することができ
る。Pyrolysis can be carried out in the flame produced by the combustion of hydrogen / air and oxygen. Instead of hydrogen, methane, butane and propane can be used.

【００１９】熱分解は更に外部加熱炉により行うことが
できる。The thermal decomposition can be further carried out by an external heating furnace.

【００２０】同様に流動床反応器、回転装置またはパル
ス反応器を使用することができる。Fluidized bed reactors, rotators or pulse reactors can likewise be used.

【００２１】本発明のインジウム−錫−酸化物は、透明
な導電性の塗料および被膜を製造するために使用するこ
とができ、その際被膜は付着性の表面（接着剤）を有す
ることができる。本発明のインジウム−錫−酸化物の他
の使用分野は平面ディスプレー、スマートウィンドーま
たは太陽電池であってもよい。The indium-tin oxide of the invention can be used for producing transparent conductive paints and coatings, the coating having an adherent surface (adhesive). . Other fields of use of the indium-tin-oxide according to the invention may be flat displays, smart windows or solar cells.

【００２２】本発明のインジウム−錫−酸化物は以下の
利点を有する。The indium-tin-oxide of the present invention has the following advantages.

【００２３】ドーピング元素に応じて生成物は所定の色
および固有の利用性を有する。Depending on the doping element, the product has a certain color and an inherent utility.

【００２４】生成物は良好な透明度を保証するために、
３００ｎｍの最大粒度を有する。In order to ensure good transparency, the product is
It has a maximum particle size of 300 nm.

【００２５】[0025]

【実施例】実施例 本発明のインジウム−錫−酸化物を製造する処理パラメ
ーターは以下の表に記載される。EXAMPLES Process parameters for making the indium-tin-oxides of the invention are set forth in the table below.

【００２６】[0026]

【表２】 [Table 2]

【００２７】得られた生成物の物理的化学的パラメータ
ーは以下の表に記載される。The physical and chemical parameters of the product obtained are set out in the table below.

【００２８】[0028]

【表３】 [Table 3]

【００２９】本発明の生成物は立方晶の酸化インジウム
および正方晶の酸化錫を有する。The product of the invention has cubic indium oxide and tetragonal tin oxide.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 クリスティアーネ ハイヤー ドイツ連邦共和国 エアクラート ヴィル ヘルムシュトラーセ ３ (72)発明者 シュティパン カトゥジック ドイツ連邦共和国 ケルクハイム ベルリ ナー リング 20 (72)発明者 ホルスト ミース ドイツ連邦共和国 カール ブルッフヴァ ルトシュトラーセ ８ (72)発明者 ペーター クレス ドイツ連邦共和国 フライゲリヒト ヘル ゲンヴェーク ７ Ｆターム(参考） 4J038 HA216 NA20    ─────────────────────────────────────────────────── ─── Continued front page    (72) Inventor Christiane Hire             Federal Republic of Germany Ekratville             Helmstrasse 3 (72) Inventor Stipan Katusik             Kerkheim Berlin, Federal Republic of Germany             Knurling 20 (72) Inventor Horst Mies             Karl Bruchva, Federal Republic of Germany             Ludstrasse 8 (72) Inventor Peter Cress             Federal Republic of Germany Freigericht Hell             Genvek 7 F-term (reference) 4J038 HA216 NA20

Claims (3)

【特許請求の範囲】[Claims] 【請求項１】 以下の物理的化学的パラメーター：透過
型電子顕微鏡（ＴＥＭ）により決定した 平均的一次粒子の大きさ １〜２００ｎｍ、 ＢＥＴ表面積（ＤＩＮ６６１３１） ０.１〜３００ｍ２／ｇ、 Ｘ線回折法（ＸＲＤ）による構造 立方晶の酸化インジウム 正方晶の酸化錫、 ＢＪＨ法（ＤＩＮ６６１３４）による メソポア ０.０３〜０.３０ｍｌ／ｇ、 マクロポア（ＤＩＮ６６１３３） １.５〜５.０ｍｌ／ｇ、 かさ密度（ＤＩＮ−ＩＳＯ７８７／ＸＩ） ５０〜２０００ｇ／ｌ を特徴とするインジウム−錫−酸化物。1. The following physical and chemical parameters: average primary particle size determined by transmission electron microscopy (TEM) 1-200 nm, BET surface area (DIN 66131) 0.1-300 m 2 / g, X-ray Structure by diffraction method (XRD) Cubic indium oxide Tetragonal tin oxide, Mesopore by BJH method (DIN66134) 0.03 to 0.30 ml / g, Macropore (DIN66133) 1.5 to 5.0 ml / g, bulk Indium-tin-oxide characterized by a density (DIN-ISO787 / XI) 50-2000 g / l. 【請求項２】 請求項１記載のインジウム−錫−酸化物
を製造する方法において、インジウム塩の溶液を錫塩の
溶液と混合し、場合により少なくとも１種のドーピング
成分の塩の溶液を添加し、この溶液混合物を噴霧し、噴
霧した溶液混合物を熱分解し、得られた生成物を排ガス
から分離することを特徴とするインジウム−錫−酸化物
の製造方法。2. A method for producing an indium-tin-oxide according to claim 1, wherein a solution of indium salt is mixed with a solution of tin salt and optionally a solution of salt of at least one doping component is added. A method for producing indium-tin-oxide, comprising spraying this solution mixture, pyrolyzing the sprayed solution mixture, and separating the obtained product from exhaust gas. 【請求項３】 透明な導電性の塗料および被膜を製造す
るための請求項１または２記載のインジウム−錫−酸化
物の使用。3. Use of the indium-tin-oxide according to claim 1 or 2 for producing transparent conductive paints and coatings.
JP2002177650A 2001-06-20 2002-06-18 Indium - tin - oxide, method for manufacturing the same and the use Withdrawn JP2003063823A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10129376A DE10129376A1 (en) 2001-06-20 2001-06-20 Indium Tin Oxide
DE10129376.3 2001-06-20

Publications (1)

Publication Number Publication Date
JP2003063823A true JP2003063823A (en) 2003-03-05

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Country Status (5)

Country Link
US (1) US20030124051A1 (en)
EP (1) EP1270511B9 (en)
JP (1) JP2003063823A (en)
AT (1) ATE303345T1 (en)
DE (2) DE10129376A1 (en)

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